CN101791429A - Preparation method of medical composite glass fiber strontium containing enhanced bone cement product - Google Patents

Preparation method of medical composite glass fiber strontium containing enhanced bone cement product Download PDF

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Publication number
CN101791429A
CN101791429A CN201010137054A CN201010137054A CN101791429A CN 101791429 A CN101791429 A CN 101791429A CN 201010137054 A CN201010137054 A CN 201010137054A CN 201010137054 A CN201010137054 A CN 201010137054A CN 101791429 A CN101791429 A CN 101791429A
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glass fiber
strontium
preparation
bone cement
strontium containing
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CN201010137054A
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李胜
李斌
李文
宋明晨
郑丽文
葛玲
陈坤宇
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李胜
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Abstract

Calcium nitrate, diammonium phosphate and urea are mixed and added with strontium phosphate to be mixed, stirred and heated, to prepare strontium containing hydroxyapatite; the hydroxyapatite is added into magnesium chloride and magnesium oxide, added with water to be dissolved, to prepare magnesium oxychloride adhesive; a hand lay-up bone pre-fabricated piece is paved with pulp and glass fiber cloth, flattened, paved uniformly and brushed with glue; and then the prefabricated outer skin is paved and compacted, the seam is sealed by plastic thin film, cured and stripped; the product is trimmed within one day after stripping, and a medical composite glass fiber strontium containing enhanced bone cement product is prepared. The composite material prepared by the invention has the advantages of uniform glass fiber dispersion and good combination of the strontium containing hydroxyapatite and a matrix interface, and biomedical composite material with very good application prospect.

Description

The preparation method of medical composite glass fiber strontium containing enhanced bone cement product
One, technical field:
The present invention relates to a kind of preparation method of strontium containing enhanced bone cement product, particularly a kind of preparation method of medical carbon fiber reinforce plastic strontium containing enhanced bone cement product.
Two, background technology:
Because reasons such as aged tendency of population, pathological changes, vehicle accident, earthquakes, annual all have a large amount of fracture patients internal fixation operation of need fracturing.Many biomaterials that are prepared from by metal and polymeric material are used for the treatment of orthopaedic disease, but there is significant defective in these materials, as: the mechanical compatibility of metal material and osseous tissue is bad, causes the loosening or dislocation of implant; Produce stress-shielding effect, cause the loose or osteanabrosis of fracture, it is silly to form bone at fracture site, is prone to the secondary fracture; The release of metal ion can cause anaphylaxis; Metal material needs second operation to take out implant; Discharge acidic materials during the polymeric material degrades of present clinical use, cause the non-bacterial inflammatory reaction, and influence the active and propagation of seed cell or somatomedin.Therefore, many research worker are devoted to develop natural polymer and the compound new bio medical material of hydroxyapatite, to satisfy the requirement of the clinical use of orthopaedics.
Hydroxyapatite is an inorganic constituents main in the nature bone, have special bone conductibility, with the good and high moisture resistance of synosteosis, be used to the clinical repair and the reconstruction of sclerous tissues.Nascent hydroapatite particles has very high absorbance and excellent biological compatibility in vivo, not only is widely used in orthopedic bone and transplants, also by the sustained release of drug delivery system.Help degraded and absorbed and stimulate new bone growth in the physiological environment small-medium size, the low-crystallinity of hydroxyapatite means high rate of dissolution, the Sr2+ ion that discharges is absorbed by osseous tissue and regenerates Sr---P inorganic mineral, thereby can promote the generation of osteoblastic adhesion, differentiation and new bone.
Therefore, develop a kind of medical composite glass fiber strontium containing enhanced bone cement product,, have great social significance and economic worth to satisfy the clinical instructions for use of orthopaedics.
Three, summary of the invention:
The purpose of this invention is to provide a kind of preparation method for preparing medical composite glass fiber strontium containing enhanced bone cement product, this method can make high-intensity strontium containing hydroxyapatite bone fracture internal fixation material---the preparation method of medical composite glass fiber strontium containing enhanced bone cement product.
The preparation method of medical composite glass fiber strontium containing enhanced bone cement product of the present invention is characterized in that described bone cement product main material weight proportion is:
Glass fibre 40 ∽ 50 grams; Strontium containing hydroxyapatite 1 ∽ 5 grams;
Magnesium oxide 2 ∽ 5 grams; Magnesium chloride 4 ∽ 10 grams;
Water 15 ∽ 25 grams; Additive 2 ∽ 5 grams;
Described strontium containing hydroxyapatite preparation method is:
A, with lime nitrate Ca (NO 3) 2, diammonium phosphate (NH 4) 2HPO 4With carbamide CO (NH 2) 22: 3: 5 by volume ∽ of solution mix at 3: 1: 6;
B, strontium salt is added in the mixed liquor, at 300 ℃ of temperature 100 ∽ reaction 1 ∽ 6 hours down;
C, reaction finish the back natural cooling, pour in the there-necked flask, leave standstill layering;
D, with the supernatant liquid elimination, residue is with flushing with clean water 2 ∽ 4 times, reuse alcohol wash 3 ∽ 5 times, sample;
E, use the alcohol burner heating, drying, after put into Muffle furnace and calcine, the time is 2 ∽ 7 hours;
Behind f, the natural cooling, after the grinding, promptly get strontium containing hydroxyapatite.
Acceptable calcium salt is on the described materia medica: strontium monophosphate SrHPO 4, strontium phosphate Sr 3(PO 4) 2, strontium carbonate SrCO 3
The preparation method of described chlorine oxygen magnesium adhesive is:
A, magnesium chloride is added water-solubleization, be made into certain density solution;
B, adding magnesium oxide mix and stir, and the time is 10min;
C, add additive in mixed liquor, behind the water reducer, fully stir, the time is 15min;
D, adding short glass fiber are made slurry.
Acceptable additive is on the described materia medica: mineral powder filler, activated alumina, ferrum oxide, copper oxide, water-soluble polyester resin, polyacrylamide; Acceptable chopped strand is on the described materia medica: glass fibre, Plant fiber, sawdust.
The denseness of described slurry is controlled with amount of water.
The preparation method of described composite glass fiber is:
A, be 0.2 ∽ 0.4mm with average thickness, diameter is that the glass fabric of 10 ∽, 13 μ m soaks with 30% hydrogen peroxide, and is standby in 100 ℃ of dry down backs of 80 ∽;
B, strontium containing hydroxyapatite is joined in the chlorine oxygen magnesium adhesive, batching fully stirs, and is standby;
C, exterior skin are made two and half skeleton shape prefabricated components;
D, stuck with paste the internal layer eyelid covering, spread plastic foamboard, pasted firmly,, shakeout, spread equal brush coating at plastic foamboard upper berth slurry, shop glass fabric;
E, then prefabricated exterior skin is spread, compacting, seam crossing is sealed with plastic sheeting;
After f, the curing, open thin film, the demoulding promptly gets medical composite glass fiber strontium containing enhanced bone cement product.
Described fiber glass reinforcement is: middle alkali fiber woven roving or grid cloth, high alkali fiber woven roving or grid cloth.
In the described blending process, the remaining slurry of gel can not be joined in the slip of the system of newly mixing.
Solidify under the described room temperature, its temperature is 50 ℃ of 10 ∽, 10 ∽ demouldings after 30 hours, and the goods finishing is finished after the demoulding, is preferably in two days.
Beneficial effect of the present invention is: strontium containing hydroxyapatite joins in the chlorine oxygen magnesium adhesive, makes glass fibre woven roving or grid cloth form the build network-like structure, becomes fine and close more, becomes tightr between layer and the layer.Simultaneously, the strontium containing hydroxyapatite granule becomes tightr, and size reduces, and can satisfy the clinical instructions for use of fracture internal fixation.
Four, specific embodiment:
Further specify the present invention below in conjunction with specific embodiment.
Embodiment 1:
1) took by weighing lime nitrate Ca (NO in 2: 3: 5 by volume 3) 2, diammonium phosphate (NH 4) 2HPO 4With carbamide CO (NH 2) 2, after the mixing, add 2 parts strontium monophosphate with volume ratio, stir 10min, form the hydroxyapatite precursor solution, react 6 hours after-filtration down for 260 ℃ in temperature, put into Muffle furnace to calcine, the time is 6 hours, behind the natural cooling, after the grinding, promptly get strontium containing hydroxyapatite;
2) 5 gram magnesium chlorides are added 20 water-solubleization of gram, be made into certain density solution, add 2 gram magnesium oxide again, after mixing stirring 10min, add the water-soluble polyester resin of 0.6 gram, behind the water reducer, fully stir 15min, add short glass fiber at last, make chlorine oxygen magnesium adhesive;
3) strontium containing hydroxyapatite 3 grams are joined in the 30 gram chlorine oxygen magnesium adhesives, batching fully stirs, and is standby;
4) exterior skin is made two and half skeleton shape prefabricated components, has stuck with paste the internal layer eyelid covering, spreads plastic foamboard, paste firmly,, shakeout, spread equal brush coating at plastic foamboard upper berth slurry, shop glass fabric, then prefabricated exterior skin is spread, compacting, seam crossing is sealed with plastic sheeting, solidifies.
5) under the room temperature, temperature is solidified down at 25 ℃, the demoulding after 19 hours, and the goods finishing is finished in two days after the demoulding, promptly gets medical composite glass fiber strontium containing enhanced bone cement product.
Embodiment 2:
1) took by weighing lime nitrate Ca (NO in 3: 3: 4 by volume 3) 2, diammonium phosphate (NH 4) 2HPO 4With carbamide CO (NH 2) 2, after the mixing, add 3 parts strontium carbonate with volume ratio, stir 10min, form the hydroxyapatite precursor solution, react 6.5 hours after-filtration down for 280 ℃ in temperature, put into Muffle furnace to calcine, the time is 7 hours, behind the natural cooling, after the grinding, promptly get strontium containing hydroxyapatite;
2) 6 gram magnesium chlorides are added 20 water-solubleization of gram, be made into certain density solution, add 2 gram magnesium oxide again, after mixing stirring 10min, add the water-soluble polyester resin and the 0.2 gram mineral powder filler of 0.5 gram, behind the water reducer, fully stir 20min, add short glass fiber at last, make chlorine oxygen magnesium adhesive;
3) strontium containing hydroxyapatite 4 grams are joined in the 30 gram chlorine oxygen magnesium adhesives, batching fully stirs, and is standby;
4) exterior skin is made two and half skeleton shape prefabricated components, has stuck with paste the internal layer eyelid covering, spreads plastic foamboard, paste firmly,, shakeout, spread equal brush coating at plastic foamboard upper berth slurry, shop glass fabric, then prefabricated exterior skin is spread, compacting, seam crossing is sealed with plastic sheeting, solidifies.
5) under the heating, temperature is solidified down at 70 ℃, the demoulding after 10 hours, and the goods finishing is finished in the demoulding one day after, promptly gets medical composite glass fiber strontium containing enhanced bone cement product.
Embodiment 3:
1) took by weighing lime nitrate Ca (NO in 3: 1: 6 by volume 3) 2, diammonium phosphate (NH 4) 2HPO 4With carbamide CO (NH 2) 2, after the mixing, add 3 parts strontium phosphate with volume ratio, stir 10min, form the hydroxyapatite precursor solution, react 6 hours after-filtration down for 300 ℃ in temperature, put into Muffle furnace to calcine, the time is 7 hours, behind the natural cooling, after the grinding, promptly get strontium containing hydroxyapatite;
2) 7 gram magnesium chlorides are added 20 water-solubleization of gram, be made into certain density solution, add 2 gram magnesium oxide again, after mixing stirring 10min, add the polyacrylamide of 0.4 gram, behind the water reducer, fully stir 20min, add short glass fiber at last, make chlorine oxygen magnesium adhesive;
3) strontium containing hydroxyapatite 4 grams are joined in the 30 gram chlorine oxygen magnesium adhesives, batching fully stirs, and is standby;
4) exterior skin is made two and half skeleton shape prefabricated components, has stuck with paste the internal layer eyelid covering, spreads plastic foamboard, paste firmly,, shakeout, spread equal brush coating at plastic foamboard upper berth slurry, shop glass fabric, then prefabricated exterior skin is spread, compacting, seam crossing is sealed with plastic sheeting, solidifies.
5) under the heating, temperature is solidified down at 60 ℃, the demoulding after 12 hours, and the goods finishing is finished in the demoulding one day after, promptly gets medical composite glass fiber strontium containing enhanced bone cement product.
Attention: in the blending process, the remaining slurry of gel can not be joined in the slip of the system of newly mixing.

Claims (10)

1. the preparation method of medical composite glass fiber strontium containing enhanced bone cement product is characterized in that described bone cement product main material weight proportion is:
Glass fibre 40 ∽ 50 grams; Strontium containing hydroxyapatite 1 ∽ 5 grams;
Magnesium oxide 2 ∽ 5 grams; Magnesium chloride 4 ∽ 10 grams;
Water 15 ∽ 25 grams; Additive 2 ∽ 5 grams;
2. the preparation method of medical composite glass fiber strontium containing enhanced bone cement product according to claim 1 is characterized in that described strontium containing hydroxyapatite preparation method is:
A, with lime nitrate Ca (NO 3) 2, diammonium phosphate (NH 4) 2HPO 4With carbamide CO (NH 2) 22: 3: 5 by volume ∽ of solution mix at 3: 1: 6;
B, strontium salt is added in the mixed liquor, at 300 ℃ of temperature 100 ∽ reaction 1 ∽ 6 hours down;
C, reaction finish the back natural cooling, pour in the there-necked flask, leave standstill layering;
D, with the supernatant liquid elimination, residue is with flushing with clean water 2 ∽ 4 times, reuse alcohol wash 3 ∽ 5 times, sample;
E, use the alcohol burner heating, drying, after put into Muffle furnace and calcine, the time is 2 ∽ 7 hours;
Behind f, the natural cooling, after the grinding, promptly get strontium containing hydroxyapatite.
3. the preparation method of medical composite glass fiber strontium containing enhanced bone cement product according to claim 1 and 2 is characterized in that acceptable calcium salt is on the described materia medica: strontium monophosphate SrHPO 4, strontium phosphate Sr 3(PO 4) 2, strontium carbonate SrCO 3
4. the preparation method of medical composite glass fiber strontium containing enhanced bone cement product according to claim 1 is characterized in that the preparation method of described chlorine oxygen magnesium adhesive is:
A, magnesium chloride is added water-solubleization, be made into certain density solution;
B, adding magnesium oxide mix and stir, and the time is 10min;
C, add additive in mixed liquor, behind the water reducer, fully stir, the time is 15min;
D, adding short glass fiber are made slurry.
5. according to the preparation method of claim 1 or 4 described medical composite glass fiber strontium containing enhanced bone cement products, it is characterized in that acceptable additive is on the described materia medica: mineral powder filler, activated alumina, ferrum oxide, copper oxide, water-soluble polyester resin, polyacrylamide; Acceptable chopped strand is on the described materia medica: glass fibre, Plant fiber, sawdust.
6. according to the preparation method of claim 1 or 4 described medical composite glass fiber strontium containing enhanced bone cement products, it is characterized in that the denseness of described slurry is controlled with amount of water.
7. the preparation method of medical composite glass fiber strontium containing enhanced bone cement product according to claim 1 is characterized in that the preparation method of described composite glass fiber is:
A, be 0.2 ∽ 0.4mm with average thickness, diameter is that the glass fabric of 10 ∽, 13 μ m soaks with 30% hydrogen peroxide, and is standby in 100 ℃ of dry down backs of 80 ∽;
B, strontium containing hydroxyapatite is joined in the chlorine oxygen magnesium adhesive, batching fully stirs, and is standby;
C, exterior skin are made two and half skeleton shape prefabricated components;
D, stuck with paste the internal layer eyelid covering, spread plastic foamboard, pasted firmly,, shakeout, spread equal brush coating at plastic foamboard upper berth slurry, shop glass fabric;
E, then prefabricated exterior skin is spread, compacting, seam crossing is sealed with plastic sheeting;
After f, the curing, open thin film, the demoulding promptly gets medical composite glass fiber strontium containing enhanced bone cement product.
8. according to the preparation method of claim 1 or 7 described medical composite glass fiber strontium containing enhanced bone cement products, it is characterized in that described fiber glass reinforcement is: middle alkali fiber woven roving or grid cloth, high alkali fiber woven roving or grid cloth.
9. according to the preparation method of claim 1 or 7 described medical composite glass fiber strontium containing enhanced bone cement products, it is characterized in that in the described blending process, the remaining slurry of gel can not be joined in the slip of the system of newly mixing.
10. according to the preparation method of claim 1 or 7 described medical composite glass fiber strontium containing enhanced bone cement products, it is characterized in that solidifying under the described room temperature, its temperature is 50 ℃ of 10 ∽, 10 ∽ demouldings after 30 hours, the goods finishing is finished after the demoulding, is preferably in two days.
CN201010137054A 2010-04-01 2010-04-01 Preparation method of medical composite glass fiber strontium containing enhanced bone cement product Pending CN101791429A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2617103C1 (en) * 2015-11-20 2017-04-20 Федеральное государственное бюджетное образовательное учреждение высшего образования "Саратовский государственный технический университет имени Гагарина Ю.А." (СГТУ имени Гагарина Ю.А.) Method for obtaining magnesium-substituted hydroxyapatite

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1562390A (en) * 2004-03-17 2005-01-12 武汉理工大学 Method for preparing artificial head bones made from composite material and for modifying surface
CN101491700A (en) * 2009-03-03 2009-07-29 陕西科技大学 Preparation method of carbon nano-tube reinforced magnesium-containing hydroxylapatite bone-cement composite material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1562390A (en) * 2004-03-17 2005-01-12 武汉理工大学 Method for preparing artificial head bones made from composite material and for modifying surface
CN101491700A (en) * 2009-03-03 2009-07-29 陕西科技大学 Preparation method of carbon nano-tube reinforced magnesium-containing hydroxylapatite bone-cement composite material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2617103C1 (en) * 2015-11-20 2017-04-20 Федеральное государственное бюджетное образовательное учреждение высшего образования "Саратовский государственный технический университет имени Гагарина Ю.А." (СГТУ имени Гагарина Ю.А.) Method for obtaining magnesium-substituted hydroxyapatite

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Application publication date: 20100804